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目的优化乙酰阿魏酰氯的合成工艺。方法先以香草醛和乙酸酐等为原料,经Perkin反应合成乙酰阿魏酸,进一步制备乙酰阿魏酰氯。按正交表L9(34)表设计考察乙酰阿魏酸和乙酰阿魏酰氯合成的影响因素,对乙酰阿魏酸合成中反应时间、PEG-400用量及投料比等因素进行优选,同时也考察乙酰阿魏酰氯合成的反应时间、反应温度及乙酰阿魏酸与氯化亚砜的摩尔比等因素对吸收率的影响。结果前者最佳工艺为A1B2C1,后者最佳工艺为A1B2C2,两步总收率达65%。结论该最佳工艺可缩短反应时间,提高生产效率,适合工业生产。
Objective To optimize the synthesis of acetyl feruloyl chloride. Methods Vanillin and acetic anhydride and other raw materials, Perkin reaction synthesis of acetyl ferulic acid, further ferulic acid acetyl chloride. According to the orthogonal table L9 (34), the factors influencing the synthesis of acetylferulic acid and acetylferrafenacyl chloride were investigated and the factors such as the reaction time, the amount of PEG-400 and the feed ratio were optimized. Acetyl ferulic acid synthesis reaction time, the reaction temperature and acetyl ferulic acid and thionyl chloride molar ratio and other factors on the absorption rate. The results of the former best for A1B2C1, the latter for the best process A1B2C2, two-step total yield of 65%. Conclusion The best process can shorten the reaction time, improve production efficiency, suitable for industrial production.